WO2015198726A1 - Highly alkali-resistant aluminum member and method for producing same - Google Patents

Highly alkali-resistant aluminum member and method for producing same Download PDF

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Publication number
WO2015198726A1
WO2015198726A1 PCT/JP2015/063478 JP2015063478W WO2015198726A1 WO 2015198726 A1 WO2015198726 A1 WO 2015198726A1 JP 2015063478 W JP2015063478 W JP 2015063478W WO 2015198726 A1 WO2015198726 A1 WO 2015198726A1
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film
aluminum
anodized film
coating layer
resistant aluminum
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PCT/JP2015/063478
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French (fr)
Japanese (ja)
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新村　仁
庸平 金谷
亮太 柿澤
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アイシン軽金属株式会社
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Publication of WO2015198726A1 publication Critical patent/WO2015198726A1/en
Priority to US15/386,408 priority Critical patent/US20170159200A1/en
Priority to US16/158,875 priority patent/US11035052B2/en

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00—Compositions for glass with special properties
    • C03C4/20—Compositions for glass with special properties for chemical resistant glass
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
    • C23D13/00—After-treatment of the enamelled articles
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
    • C23D3/00—Chemical treatment of the metal surfaces prior to coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
    • C23D5/00—Coating with enamels or vitreous layers
    • C23D5/02—Coating with enamels or vitreous layers by wet methods
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/14—Producing integrally coloured layers
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • C25D11/246—Chemical after-treatment for sealing layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2202/00—Metallic substrate
    • B05D2202/20—Metallic substrate based on light metals
    • B05D2202/25—Metallic substrate based on light metals based on Al
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/20—Electrolytic after-treatment
    • C25D11/22—Electrolytic after-treatment for colouring layers
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • C25D11/243—Chemical after-treatment using organic dyestuffs

Definitions

  • the present invention relates to a member made of aluminum or aluminum alloy having excellent alkali resistance.
  • Patent Documents 1 and 2 disclose a technique in which a silane coupling agent is applied onto an anodized film and then coated thereon.
  • Patent Document 3 discloses a technique in which an anodized film is immersed in a mixed alcohol solution of alkoxysilane and HCl. However, the purpose of this technique is to fill SiO 2 in the fine pores of the anodized film, and it is not possible to form a coating layer on the anodized film.
  • An object of the present invention is to provide an aluminum and aluminum alloy member having improved alkali resistance of an anodized film.
  • the highly alkali-resistant aluminum member according to the present invention has an anodized film layer on the surface of aluminum or an aluminum alloy, and has a coating layer having a siloxane glass component of 90% by mass or more on the anodized film layer.
  • the coating layer has a thickness of 0.5 to 5.0 ⁇ m and an adhesion amount of 0.4 to 5.0 g / m 2 .
  • 90 mass% or more of the siloxane glass component means a coating layer in which the glass-like component having a Si—O—Si siloxane bond accounts for 90 mass% or more.
  • a coating layer can be obtained by applying a high-concentration paint having an alkoxysiloxane compound of 50% by mass or more on the anodized film and drying it. Alkoxysiloxane is hydrolyzed on the coated surface and cured at room temperature.
  • the siloxane glass component is 90% by mass or more, a transparent and hard coating layer is obtained.
  • the siloxane glass component is further 95% by mass or more, the transparency is further increased.
  • the anodized film when the anodized film is a sulfuric acid electrolytic film or an oxalic acid electrolytic film that has been subjected to hot water washing treatment or semi-sealing treatment, adhesion of the coating layer of siloxane glass is improved.
  • the anodized film may be a colored film.
  • the method for producing a highly alkali-resistant aluminum member according to the present invention comprises a step of forming an anodic oxide film having a thickness of 5 to 20 ⁇ m on the surface of aluminum or an aluminum alloy, and then a hot water of 70 to 85 ° C. for 5 to 30 minutes. It has a step of performing a hot water washing process or a semi-sealing process, and then applying and drying an alkoxysiloxane paint.
  • the sulfuric acid electrolytic film refers to forming an anodic oxide film in a sulfuric acid aqueous solution
  • the oxalic acid electrolytic film refers to an oxalic acid aqueous solution used as an electrolytic solution.
  • coloring includes so-called secondary electrolytic coloring and dyeing.
  • the aluminum or aluminum alloy member according to the present invention has a coating layer made of siloxane glass on the anodized film, it is excellent not only in corrosion resistance in an acidic environment but also in alkali resistance. Moreover, it is transparent and glossy, and can maintain the texture of the conventional anodized film and the metallic luster of the aluminum surface.
  • the manufacture example of the aluminum or aluminum alloy member which concerns on this invention, and its evaluation result are demonstrated.
  • the aluminum alloy extruded material was subjected to electrolytic treatment in an aqueous sulfuric acid solution, and an anodized film was formed according to a conventional method.
  • the film thickness was 10 ⁇ m.
  • it was immersed in warm water of 80 ° C. to 95 ° C. for 5 to 20 minutes.
  • an alkoxysiloxane paint was applied and dried at room temperature.
  • the product name “Top Notch Coat TN-7000” manufactured by JSP Co., Ltd. was used as the paint containing 50% by mass or more of the alkoxysiloxane used in the evaluation.
  • coat changes thickness, The thickness of the glassy coating layer after drying was shown in the table
  • targets for adhesion and alkali resistance were set as follows so that they could be applied to automobile exterior parts.
  • ⁇ Adhesion> After immersing the test piece in pure water at 40 ° C. for 360 hours, a 1 mm square grid was put in the vitreous coating layer, and a peeling test using a cellophane tape was carried out.
  • ⁇ Alkali resistance> The test piece was immersed in a 1 / 10N aqueous sodium hydroxide solution (20 ° C.) for 20 minutes, and then washed and dried. As a result, the case where no discoloration was observed was evaluated as “ ⁇ ”.
  • Example 1 and Comparative Example 2 the adhesion was evaluated as “Good” as shown in Example 1 and Comparative Example 2 under conditions where hot water immersion after anodized film treatment was 80 ° C. ⁇ 5 minutes.
  • the adhesion was insufficient. From this, the adhesiveness decreases as the degree of sealing of the anodized film progresses, so the level of hot water for the purpose of washing the acid remaining in the anodized film, or the case where the sealing does not progress completely. It can be said that the sealing level is good.
  • the hot water washing treatment or semi-sealing treatment is preferably immersed in warm water at 70 to 85 ° C. for 5 to 30 minutes.
  • hot water of 75 to 85 ° C. is preferable.
  • the target could not be cleared when the thickness of the glassy coating layer of Comparative Example 2 was 0.4 ⁇ m.
  • the adhesion amount in this range was 0.4 to 5.0 g / m 2 .
  • the sulfuric acid electrolytic film using an aqueous sulfuric acid solution was 10 ⁇ m.
  • the film thickness is preferably in the range of 5 to 20 ⁇ m, and the oxalic acid electrolytic film having the same film thickness. It may be.
  • the aluminum alloy material may be subjected to mechanical finishing such as buffing or chemical finishing such as chemical polishing or electrolytic polishing.
  • the surface treatment according to the present invention is excellent in alkali resistance while maintaining the radiance.
  • the anodized film may be colored by secondary electrolytic coloring or dyeing.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Application Of Or Painting With Fluid Materials (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Paints Or Removers (AREA)

Abstract

[Problem] The purpose of the present invention is to provide an aluminum or aluminum alloy member wherein the alkali resistance of an anodic oxide coating film is improved. [Solution] A highly alkali-resistant aluminum member which is characterized in that: an anodic oxide coating film is disposed on the surface of an aluminum or aluminum alloy; a coating layer having a siloxane glass component of 90% by mass or more is disposed on the anodic oxide coating film; and the coating layer has a thickness of 0.5-5.0 μm and an adhesion amount of 0.4-5.0 g/m2.

Description

高耐アルカリ性アルミニウム部材及びその製造方法High alkali-resistant aluminum member and method for producing the same
　本発明は、耐アルカリ性に優れたアルミニウム又はアルミニウム合金からなる部材に関する。 The present invention relates to a member made of aluminum or aluminum alloy having excellent alkali resistance.
　アルミニウム又はアルミニウム合金は、そのままで外装部品として使用するには耐食性が不充分であることから、陽極酸化皮膜処理が行われている。
　この種の陽極酸化皮膜は、酸性に対しての耐食性は相対的に優れるものの、アルカリ性に対しては表面が白化しやすく、例えば自動車等の外装部品に適用するには不充分であった。
　建材の分野にあっては、陽極酸化皮膜を形成後に電着塗装を施すことで耐アルカリ性を向上させているが、この電着塗膜はキズ付きやすく、この種のアルミニウム材を自動車部品に用いると洗車時にキズが付き、剥がれやすい問題がある。
　また、特許文献１，２には、陽極酸化皮膜の上にシランカップリング剤を塗布し、その上に塗装する技術を開示するが、ここでシランカップリング剤は、塗膜の密着性を向上させるのが目的であって、シランカップリング剤のみでは耐食性が不充分である。
　特許文献３には、アルコキシシランとＨＣｌの混合アルコール溶液に陽極酸化皮膜を浸漬する技術を開示する。
　しかし、同技術は陽極酸化皮膜の微細孔中にＳｉＯ２を充填させるのが目的であり、陽極酸化皮膜の上にコーティング層を形成できるものではない。 Since aluminum or an aluminum alloy has insufficient corrosion resistance to be used as an exterior part as it is, an anodized film treatment is performed.
This type of anodized film is relatively excellent in corrosion resistance against acidity, but the surface is easily whitened against alkalinity, and is insufficient for application to exterior parts such as automobiles.
In the field of building materials, alkali resistance is improved by applying electrodeposition coating after forming an anodized film, but this electrodeposition coating film is easily scratched, and this kind of aluminum material is used for automobile parts. And there is a problem that it gets scratched during car wash and easily peels off.
Patent Documents 1 and 2 disclose a technique in which a silane coupling agent is applied onto an anodized film and then coated thereon. Here, the silane coupling agent improves the adhesion of the coating film. The purpose is to make the silane coupling agent alone, the corrosion resistance is insufficient.
Patent Document 3 discloses a technique in which an anodized film is immersed in a mixed alcohol solution of alkoxysilane and HCl.
However, the purpose of this technique is to fill SiO 2 in the fine pores of the anodized film, and it is not possible to form a coating layer on the anodized film.
日本国特許第４２４８８１８号公報Japanese Patent No. 4248818 日本国特許第４１７６５８１号公報Japanese Patent No. 4176581 日本国特開平６－３１６７８７号公報Japanese Unexamined Patent Publication No. 6-316787
　本発明は、陽極酸化皮膜の耐アルカリ性を向上させたアルミニウム及びアルミニウム合金部材の提供を目的とする。 An object of the present invention is to provide an aluminum and aluminum alloy member having improved alkali resistance of an anodized film.
　本発明に係る高耐アルカリ性アルミニウム部材は、アルミニウム又はアルミニウム合金の表面に陽極酸化皮膜層を有し、前記陽極酸化皮膜層の上に、シロキサンガラス成分が９０質量％以上のコーティング層を有し、前記コーティング層は、厚み０．５～５．０μｍ，付着量０．４～５．０ｇ／ｍ２であることを特徴とする。 The highly alkali-resistant aluminum member according to the present invention has an anodized film layer on the surface of aluminum or an aluminum alloy, and has a coating layer having a siloxane glass component of 90% by mass or more on the anodized film layer. The coating layer has a thickness of 0.5 to 5.0 μm and an adhesion amount of 0.4 to 5.0 g / m 2 .
　ここで、シロキサンガラス成分が９０質量％以上とは、Ｓｉ－Ｏ－Ｓｉシロキサン結合を有するガラス状の成分が９０質量％以上占めるコーティング層であることをいう。
　このようなコーティング層は、アルコキシシロキサン化合物が５０質量％以上の高濃度の塗料を陽極酸化皮膜の上に塗布し、乾燥させることで得られる。
　アルコキシシロキサンは、塗布面にて加水分解し、常温硬化する。
　シロキサンガラス成分が９０質量％以上占めると、透明で硬い皮膜層となる。
　シロキサンガラス成分がさらに９５質量％以上となると、より透明度が増す。 Here, 90 mass% or more of the siloxane glass component means a coating layer in which the glass-like component having a Si—O—Si siloxane bond accounts for 90 mass% or more.
Such a coating layer can be obtained by applying a high-concentration paint having an alkoxysiloxane compound of 50% by mass or more on the anodized film and drying it.
Alkoxysiloxane is hydrolyzed on the coated surface and cured at room temperature.
When the siloxane glass component is 90% by mass or more, a transparent and hard coating layer is obtained.
When the siloxane glass component is further 95% by mass or more, the transparency is further increased.
　本発明において、陽極酸化皮膜は湯洗処理又は半封孔処理された硫酸電解皮膜又はシュウ酸電解皮膜であると、シロキサンガラスのコーティング層の密着性が向上する。
　また、本発明においては、陽極酸化皮膜は着色皮膜であってよい。 In the present invention, when the anodized film is a sulfuric acid electrolytic film or an oxalic acid electrolytic film that has been subjected to hot water washing treatment or semi-sealing treatment, adhesion of the coating layer of siloxane glass is improved.
In the present invention, the anodized film may be a colored film.
　本発明に係る高耐アルカリ性アルミニウム部材の製造方法は、アルミニウム又はアルミニウム合金の表面に厚み５～２０μｍの陽極酸化皮膜を形成するステップと、次に７０～８５℃の温水にて５～３０分間の湯洗処理又は半封孔処理するステップと、次に、アルコキシシロキサン塗料を塗布及び乾燥するステップとを有することを特徴とする。
　ここで、硫酸電解皮膜とは、硫酸水溶液中で陽極酸化皮膜を形成することをいい、シュウ酸電解皮膜とは、シュウ酸水溶液を電解液に用いたものをいう。
　また、陽極酸化皮膜を形成した後に着色処理し、次に前記湯洗処理又は半封孔処理するステップを有するようにしてもよい。
　着色には、いわゆる二次電解着色や染色が含まれる。 The method for producing a highly alkali-resistant aluminum member according to the present invention comprises a step of forming an anodic oxide film having a thickness of 5 to 20 μm on the surface of aluminum or an aluminum alloy, and then a hot water of 70 to 85 ° C. for 5 to 30 minutes. It has a step of performing a hot water washing process or a semi-sealing process, and then applying and drying an alkoxysiloxane paint.
Here, the sulfuric acid electrolytic film refers to forming an anodic oxide film in a sulfuric acid aqueous solution, and the oxalic acid electrolytic film refers to an oxalic acid aqueous solution used as an electrolytic solution.
Moreover, after forming an anodic oxide film, you may make it have a coloring process, and the step which performs the said hot-water washing process or a semi-sealing process next.
Coloring includes so-called secondary electrolytic coloring and dyeing.
　本発明に係るアルミニウム又はアルミニウム合金部材は、陽極酸化皮膜の上にシロキサンガラスからなるコーティング層を有するので、酸性環境下における耐食性のみならず、耐アルカリ性にも優れる。
　また、透明で艶があり、従来の陽極酸化皮膜の質感やアルミニウム表面の金属光沢を維持できる。 Since the aluminum or aluminum alloy member according to the present invention has a coating layer made of siloxane glass on the anodized film, it is excellent not only in corrosion resistance in an acidic environment but also in alkali resistance.
Moreover, it is transparent and glossy, and can maintain the texture of the conventional anodized film and the metallic luster of the aluminum surface.
表面処理条件とその評価結果を示す。The surface treatment conditions and the evaluation results are shown.
　本発明に係るアルミニウム又はアルミニウム合金部材の製造例及びその評価結果を説明する。
　アルミニウム合金の押出材を硫酸水溶液中にて電解処理し、常法に従い陽極酸化皮膜を形成した。
　皮膜の膜厚は、１０μｍであった。
　次に図１の表に示すように８０℃～９５℃の温水に５～２０ｍｉｎ浸漬処理した。
　上記の温水処理した後に乾燥させた後、アルコキシシロキサン塗料を塗布し、常温乾燥させた。
　ここで、評価に用いたアルコキシシロキサンが５０質量％以上含有する塗料は、株式会社ジェイ・エス・ピー社製の商品名「トップノッチコートＴＮ－７０００」を用いた。
　なお、塗布する量は厚みを変化させ、乾燥した後のガラス質コーティング層の厚みを図１の表に示した。 The manufacture example of the aluminum or aluminum alloy member which concerns on this invention, and its evaluation result are demonstrated.
The aluminum alloy extruded material was subjected to electrolytic treatment in an aqueous sulfuric acid solution, and an anodized film was formed according to a conventional method.
The film thickness was 10 μm.
Next, as shown in the table of FIG. 1, it was immersed in warm water of 80 ° C. to 95 ° C. for 5 to 20 minutes.
After the above hot water treatment and drying, an alkoxysiloxane paint was applied and dried at room temperature.
Here, the product name “Top Notch Coat TN-7000” manufactured by JSP Co., Ltd. was used as the paint containing 50% by mass or more of the alkoxysiloxane used in the evaluation.
In addition, the quantity to apply | coat changes thickness, The thickness of the glassy coating layer after drying was shown in the table | surface of FIG.
　品質目標としては、自動車の外装部品に適用できるように密着性及び耐アルカリ性の目標を下記のとおり設定した。
＜密着性＞
　試験片を４０℃の純水に３６０時間浸漬した後に、ガラス質コーティング層に１ｍｍマス目の碁盤目を入れ、セロハンテープによる剥がれ試験を実施し、剥がれ０／１００を評価「○」とした。
＜耐アルカリ性＞
　試験片を１／１０Ｎの水酸化ナトリウム水溶液（２０℃）に２０分間浸漬し、その後洗浄乾燥した。
　これにより、変色が認められないものを評価「○」とした。 As quality targets, targets for adhesion and alkali resistance were set as follows so that they could be applied to automobile exterior parts.
<Adhesion>
After immersing the test piece in pure water at 40 ° C. for 360 hours, a 1 mm square grid was put in the vitreous coating layer, and a peeling test using a cellophane tape was carried out.
<Alkali resistance>
The test piece was immersed in a 1 / 10N aqueous sodium hydroxide solution (20 ° C.) for 20 minutes, and then washed and dried.
As a result, the case where no discoloration was observed was evaluated as “◯”.
　図１の表に示した結果から、次のことが明らかになった。
　（１）陽極酸化皮膜処理後の温水浸漬が８０℃×５分の条件で実施例１，比較例２で示すように密着性が評価「○」となった。
　これに対して温水浸漬９０℃×２０分では、比較例３に示すように密着性が不充分であった。
　このことから、陽極酸化皮膜の封孔度が進行すると密着性が低下することから、陽極酸化皮膜中に残る酸の洗浄を目的とした湯洗レベル、又は封孔が完全に進行していない半封孔レベルが良いと言える。
　よって、湯洗処理又は半封孔処理は、７０～８５℃の温水に５～３０分間浸漬するのが好ましい。
　なお、浸漬時間を５～２０分間程度にするには、７５～８５℃の温水がよい。 From the results shown in the table of FIG.
(1) As shown in Example 1 and Comparative Example 2, the adhesion was evaluated as “Good” as shown in Example 1 and Comparative Example 2 under conditions where hot water immersion after anodized film treatment was 80 ° C. × 5 minutes.
On the other hand, in the case of 90 ° C. × 20 minutes immersion in warm water, as shown in Comparative Example 3, the adhesion was insufficient.
From this, the adhesiveness decreases as the degree of sealing of the anodized film progresses, so the level of hot water for the purpose of washing the acid remaining in the anodized film, or the case where the sealing does not progress completely. It can be said that the sealing level is good.
Therefore, the hot water washing treatment or semi-sealing treatment is preferably immersed in warm water at 70 to 85 ° C. for 5 to 30 minutes.
In order to set the immersion time to about 5 to 20 minutes, hot water of 75 to 85 ° C. is preferable.
　次に耐アルカリ性については、比較例２のガラス質コーティング層の厚み０．４μｍでは目標をクリアーすることができなかったから、このガラス質コーティング層は０．５～５．０μｍの範囲がよい。
　この範囲の付着量は、０．４～５．０ｇ／ｍ２であった。 Next, with respect to alkali resistance, the target could not be cleared when the thickness of the glassy coating layer of Comparative Example 2 was 0.4 μm.
The adhesion amount in this range was 0.4 to 5.0 g / m 2 .
　本実施例は、硫酸水溶液を用いた硫酸電解皮膜１０μｍであったが、自動車の外装部品として使用するには、皮膜厚さが５～２０μｍの範囲が好ましく、同様の膜厚のシュウ酸電解皮膜であってもよい。
　また、アルミニウム合金素材は、バフ研磨等の機械的仕上げや化学研磨，電解研磨等の化学的仕上げが施されていてもよい。
　このようにアルミニウム素材を光輝仕上げしてあると、本発明に係る表面処理にて光輝性を維持しつつ、耐アルカリ性に優れる。
　また、陽極酸化皮膜に二次電解着色や染色により、着色を施してあってもよい。 In this example, the sulfuric acid electrolytic film using an aqueous sulfuric acid solution was 10 μm. However, for use as an automobile exterior part, the film thickness is preferably in the range of 5 to 20 μm, and the oxalic acid electrolytic film having the same film thickness. It may be.
The aluminum alloy material may be subjected to mechanical finishing such as buffing or chemical finishing such as chemical polishing or electrolytic polishing.
Thus, when the aluminum material is brilliantly finished, the surface treatment according to the present invention is excellent in alkali resistance while maintaining the radiance.
The anodized film may be colored by secondary electrolytic coloring or dyeing.

Claims (3)

  1. 　アルミニウム又はアルミニウム合金の表面に陽極酸化皮膜層を有し、
    前記陽極酸化皮膜層の上に、シロキサンガラス成分が９０質量％以上のコーティング層を有し、
    前記コーティング層は、厚み０．５～５．０μｍ，付着量０．４～５．０ｇ／ｍ２であることを特徴とする高耐アルカリ性アルミニウム部材。     Having an anodized film layer on the surface of aluminum or aluminum alloy;
    On the anodized film layer, a siloxane glass component has a coating layer of 90% by mass or more,
    The high alkali-resistant aluminum member, wherein the coating layer has a thickness of 0.5 to 5.0 μm and an adhesion amount of 0.4 to 5.0 g / m 2 .
  2. 　前記陽極酸化皮膜は湯洗処理又は半封孔処理された硫酸電解皮膜又はシュウ酸電解皮膜であることを特徴とする請求項１記載の高耐アルカリ性アルミニウム部材。 2. The highly alkali-resistant aluminum member according to claim 1, wherein the anodized film is a sulfuric acid electrolytic film or an oxalic acid electrolytic film which has been subjected to a hot water washing treatment or a semi-sealing treatment.
  3. 　前記陽極酸化皮膜は着色皮膜であることを特徴とする請求項１又は２記載の高耐アルカリ性アルミニウム部材。 3. The highly alkaline resistant aluminum member according to claim 1, wherein the anodized film is a colored film.
PCT/JP2015/063478 2014-06-25 2015-05-11 Highly alkali-resistant aluminum member and method for producing same WO2015198726A1 (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06306333A (en) * 1993-04-26 1994-11-01 Toshiba Silicone Co Ltd Method for bonding millable silicone rubber
JPH08120490A (en) * 1994-10-25 1996-05-14 Matsushita Electric Ind Co Ltd Aluminum oxidized film and its production
JPH11229187A (en) * 1997-12-11 1999-08-24 Kobe Steel Ltd Substrate for electronic material excellent in insulating property and its production

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4431489A (en) * 1983-03-31 1984-02-14 Kaiser Aluminum & Chemical Corporation Coloring process for anodized aluminum products
JPH06316787A (en) 1993-04-28 1994-11-15 Kojundo Chem Lab Co Ltd Treatment of surface of anodized alminum layer
JPH08337654A (en) * 1995-06-14 1996-12-24 Matsushita Electric Ind Co Ltd Production of chemisorption film, and chemisorption fluid used therefor
JPH1119587A (en) * 1997-06-27 1999-01-26 Aisin Keikinzoku Kk Surface treating method for aluminum alloy
EP1087038A1 (en) * 1999-09-23 2001-03-28 Clariant International Ltd. Process for dyeing oxide layers on aluminum
JP2001335989A (en) * 2000-05-31 2001-12-07 Kobe Steel Ltd Anodic oxidized al material having excellent corrosion resistance, method for manufacturing the same and al parts for plasma atmosphere same
DE10063739B4 (en) * 2000-12-21 2009-04-02 Ferro Gmbh Substrates with self-cleaning surface, process for their preparation and their use
JP2002212787A (en) * 2001-01-12 2002-07-31 Kobe Steel Ltd HIGHLY CORROSION RESISTING Al ALLOY MEMBER AND PRODUCTION METHOD THEREFOR
JP4248818B2 (en) 2002-08-07 2009-04-02 三菱アルミニウム株式会社 Method for producing surface-treated aluminum material
JP4176581B2 (en) 2003-07-02 2008-11-05 三菱アルミニウム株式会社 Surface-treated aluminum material and aluminum molded body
JP2006111894A (en) * 2004-10-12 2006-04-27 Fuji Heavy Ind Ltd Surface treatment method for aluminum alloy
DE102005027789A1 (en) * 2005-06-15 2006-12-21 Nano-X Gmbh Alkali-stable sol-gel coating
CN101885257B (en) 2010-06-25 2012-12-05 山东大学 Method for preparing transparent organic hydrophobic coating on surface of aluminum plate
DE102012204636A1 (en) * 2012-03-22 2013-09-26 Nanogate Ag Treatment of anodized surface

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06306333A (en) * 1993-04-26 1994-11-01 Toshiba Silicone Co Ltd Method for bonding millable silicone rubber
JPH08120490A (en) * 1994-10-25 1996-05-14 Matsushita Electric Ind Co Ltd Aluminum oxidized film and its production
JPH11229187A (en) * 1997-12-11 1999-08-24 Kobe Steel Ltd Substrate for electronic material excellent in insulating property and its production

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